L-环己基甘氨酸工业品中L-苯甘氨酸的HPLC测定

Determination of L-phenylglycine in L-cyclohexylglycine for industrial use by HPLC

建立一种测定L-环己基甘氨酸工业品中L-苯甘氨酸含量的高效液相色谱（HPLC）法。色谱柱为Agela Innoval C18（250 mm×4.6 mm×5μm）,采用乙腈-20 mmol/L磷酸二氢钾溶液（v∶v=8∶92）为流动相（p H 5.0）。L-苯甘氨酸在质量浓度为1.25×10-4~0.5 mg/m L时线性关系良好,相关系数r2为0.998 7。实际样品中L-苯甘氨酸日内和日间测定精密度分别为1.2%和2.7%,回收率为102.7%。所建立的HPLC方法能够很好地提供L-环己基甘氨酸样品中相关杂质L-苯甘氨酸的含量信息,并可反映出L-环己基甘氨酸的原料转化率,从而有效地指导其生产工艺的控制。

A high performance liquid chromatography-UV detection was established for the determination of L-phenylglycine in L-cyclohexylglycine industrial products. The separation was carried out on Agela lnnoval C18 column （250mm×4.6mm×5 μm）, using acetonitrile-20mmol/L KH2PO4 aqueous solution （pH 5.0）, 8：92 （v：v） as mobile phase in an isocratic elution. The linear range of L-phenylglycine was 1.25×10-0.5mg/mL and the correlation coefficient r2was 0.998 7. Good reproducibility was obtained in real industrial samples with intra-and inter-day relative standard deviations （RSDs） of 1.2% and 2.7%, respectively. The average recovery was determined as 102.7%. The established method provides information of the content of related impurity L- phenylglycine in the industrial L-cyclohexylglycine. The method can also reflect the conversion of reactants so as to provide information for the production process control of L-cyclohexylglyeine.